摘要
大量用于预防和治疗细菌和真菌性等疾病的抗生素药物未经完全代谢后最终进入自然水体,对饮用水源水质安全构成潜在威胁.为快速测定饮用水源水体中的抗生素残留,保障饮水安全,本论文建立一种固相萃取-高效液相色谱串联质谱法测定13种抗生素的分析方法.采用OASIS■HLB小柱对水样进行固相萃取富集和净化,以甲醇和0.5%的甲酸(含5 mmol·L^(-1)乙酸铵)水溶液为流动相,经Kinetex■C18色谱柱分离后采用三重四极杆串联质谱多反应监测模式分析.该方法检出限为0.05—1.66 ng·L^(-1),定量限为0.17—5.52 ng·L^(-1),回收率为70.2%—121.5%,相对标准偏差为1.1%—13.5%.该方法准确度高,灵敏度高,适用于饮用水源源水中痕量抗生素残留的测定.方法成功应用于厦门市饮用水源源水中抗生素残留分析,共检出7种抗生素,浓度范围为ND—32.6 ng·L^(-1).
Antibiotics are used for the prevention and treatment of bacterial and fungal diseases.The residual antibiotics end up in natural water bodies,leading to safe drinking water quality.In order to rapid determination antibiotic residues in drinking water and ensure the safety of drinking water,an analytical method was developed for the simultaneous determination of 13 antibiotics residues in 4 classes in waters of drinking water source by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry.The samples were concentrated and purified with OASIS■HLB cartridge.Gradient elution was performed using methanol as mobile phase B and 0.5%formic acid water containing 5 mmol·L^(-1) ammonium acetate as mobile phase A.Samples were analyzed by means of multiple reaction monitoring(MRM)through the mass separation by Kinetex■C18 column.The detection limits and quantization limits for the 13 antibiotics were0.05—1.66 ng·L^(-1) and 0.17—5.52 ng·L^(-1),respectively.The recoveries ranged from 70.2%to 121.5%with relative standard deviations of 1.1%—13.5%.The method has high sensitivity,high efficiency which can be used for simultaneous determination of antibiotics residues in source water of drinking water sources at trace level.The method was successfully applied to analysis of antibiotics residue in source water in Xiamen.7 antibiotics were detected,and the concentrations ranged from not detected to 32.6 ng·L^(-1).
作者
廖杰
李青松
LIAO Jie;LI Qingsong(The Key Laboratory of Water Resources Utilization and Protection of Xiamen,School of Environmental Science and Engineering,Xiamen University of Technology,Xiamen,361024,China)
出处
《环境化学》
CAS
CSCD
北大核心
2022年第5期1538-1547,共10页
Environmental Chemistry
基金
国家自然科学基金(51878582)资助。
关键词
高效液相色谱串联质谱法
抗生素
固相萃取
饮用水源
high performance liquid chromatography-tandem mass spectrometry
antibiotic
solid phase extraction
drinking water source
